調整 Ni-P 共觸媒濃度與電沉積時間之鍺摻雜α-Fe2O3光陽極應用於 5-羥甲基糠醛選擇性氧化為 2,5-呋喃二甲酸

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吳律旻(Lu-Min Wu) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

調整 Ni-P 共觸媒濃度與電沉積時間之鍺摻雜α-Fe2O3光陽極應用於 5-羥甲基糠醛選擇性氧化為 2,5-呋喃二甲酸
(Tuning the Precursor Concentration and Deposition Time of Nickel Phosphate Co-catalyst on Germanium doped α-Fe2O3 Photoanode for Selective oxidation of 5-Hydroxymethylfurfural to 2,5-Furandicarboxylic acid)

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至系統瀏覽論文 (2027-9-23以後開放)

摘要(中)

在光電化學 (Photoelectrochemical, PEC) 當中光陽極產氧並不符合動力學的趨勢，因此利用生質 (Biomass) 的選擇性氧化加以取代，透過反應得到具高附加價值的生質化學品，希望能代替原本的石化產品。本實驗選用地表含量豐富、光電表現穩定且無毒的α-Fe2O3作為光陽極，適合使用於長時間的氧化反應。透過水熱法製備α-Fe2O3薄膜，其中摻雜鍺 (Ge) 可以增加電子濃度，讓α-Fe2O3的導電度與載子遷移率增加，在光電化學上有更好的表現。反應物方面選用木質素衍生物5-羥甲基糠醛 (5- Hydroxymethylfurfural, HMF)，透過氧化生成的2,5-呋喃二甲酸 (2,5-Furandicarboxylic acid, FDCA) 可聚合成聚2,5-呋喃二甲酸乙二酯 (Polyethylene 2,5-furandicarboxylate, PEF) 樹脂，可望能取代目前常用的聚對苯二甲酸乙二酯 (Polyethylene terephthalate, PET)。
透過裝載共觸媒幫忙捕捉電洞，降低再結合的機率，可以進一步幫助光電化學與氧化表現，透過改變電沉積時間與前驅液濃度裝載Nickel Phosphate (Ni-P)，再利用四甲基哌啶氧化物 (2,2,6,6-Tetramethylpiperidine-1-oxyl, TEMPO) 輔助催化，促使HMF轉化為FDCA。結果顯示在選擇性氧化表現上以電沉積30分鐘，前驅液中鎳與磷酸根莫爾比為15比200時有最佳表現，與未裝載的情況相比，在反應12小時後FDCA的選擇率從35.4 % 提升至67.1 %，產率也從11.8 %上升至35.7 %，HMF的轉化率也有61.1 %，不僅如此，光電流也從0.51 mA上升至0.79 mA。綜上所述，作為HMF選擇性氧化的光陽極，α-Fe2O3是十分具潛力的選擇，Ni-P作為共觸媒能有效的幫助FDCA的生成，在反應中佔有重要的角色。

摘要(英)

Anode oxygen evolution reaction ( OER ) is not kinetically favorable in photoelectrochemical ( PEC ) cell. Thus, it is feasible to replace OER by oxidizing the biomass into high value-added chemicals. In this work, we use α-Fe2O3 as the photoanode which is non-toxic, stable in PEC system and earth-abundant. First, Ge-doped α-Fe2O3 thin film was synthesized using hydrothermal method with germanium oxide (GeO2) adding into iron oxide precursor. Ge doping can increase electron concentration, conductivity and carrier mobility of α-Fe2O3. Therefore, it can improve the performance in PEC system. 5-Hydroxymethylfurfural (HMF) was used as the reactant and it was oxidized to 2,5-Furandicarboxylic acid (FDCA) which can be polymerized into Polyethylene 2,5-furandicarboxylate (PEF).
By loading the co-catalyst to capture holes and reduce the recombination, it can further enhance the photoelectrochemical and oxidation performance. Load Nickel Phosphate (Ni-P) by changing the electrodeposition time and the concentration of the precursor, and add 2,2,6,6-Tetramethylpiperidine-1-oxyl (TEMPO) as a mediator which can facilitate the selective oxidation of HMF. The results show that for selective oxidation, the electrodeposition for 30 minutes and the molar ratio of nickel to phosphate in the precursor are the best at 15:200. Compared with the unloaded case, the selectivity of FDCA increased from 35.4 % to 67.1 % after 12 hours of reaction. The yield also increased from 11.8 % to 41.0 %, and the conversion of HMF also achieved 61.1 %. Moreover, the photocurrent increased from 0.51 mA to 0.79 mA. In conclusion, α-Fe2O3 is a promising chemical as a photoanode for the selective oxidation of HMF, and Ni-P, as a co-catalyst, can effectively help the formation of FDCA and plays a big part in the reaction.

關鍵字(中)

★ 光電化學
★ 氧化鐵
★ 選擇性氧化

關鍵字(英)

★ Photoelectrochemical
★ α-Fe2O3
★ Selective oxidation

論文目次

摘要 i
Abstract ii
誌謝 iv
目錄 v
圖目錄 ix
表目錄 xv
第一章、緒論 1
1-1前言 1
1-2 光觸媒發展 3
1-3研究動機 5
第二章、文獻回顧 7
2-1半導體光觸媒 7
2-1-1半導體 7
2-1-2 光觸媒 9
2-1-3 半導體與電解液界面 10
2-2 光電化學分解水 12
2-3 α - Fe2O3 半導體光觸媒 15
2-3-1 α - Fe2O3 簡介 15
2-3-2 α - Fe2O3 光電化學特性與缺點 16
2-3-3 α - Fe2O3改善方法 18
2-3-3-1 型態優化 18
2-3-3-2 元素摻雜 19
2-3-3-3 共觸媒 20
2-3-3-4 鈍化層 22
2-3-3-5 基板與光觸媒的界面處理 22
2-4 光催化生質與選擇性氧化 24
2-4-1 光催化生質 24
2-4-2 選擇性氧化 27
2-5 電化學交流阻抗頻譜 30
2-5-1 EIS基礎理論 30
2-5-2 等效電路模型 30
第三章、研究方法 34
3-1 實驗藥品 34
3-2實驗儀器 37
3-3 實驗步驟 42
3-3-1 光電極製備 42
3-3-1-1 α-Fe2O3試片 42
3-3-1-2 Ge doped α-Fe2O3試片 44
3-3-1-3 Ni-P共觸媒裝載 44
3-3-2 光電化學量測 45
3-3-3 選擇性氧化 46
3-3-3-1 反應系統 46
3-3-3-2 液相層析分析 47
3-3-4 EIS量測 48
第四章、結果與討論 49
4-1 α-Fe2O3光電極 49
4-2 Ge doped α-Fe2O3光電極 52
4-2-1 基本性質分析 52
4-2-2光電化學分析 58
4-3 Ni-P共觸媒裝載 59
4-3-1 更變前驅液濃度之Ni-P裝載 59
4-3-1-1 基本性質分析 59
4-3-1-2 光電化學分析 67
4-3-1-3 HMF氧化反應 69
4-3-1-4 選擇性氧化檢量線 71
4-3-1-5 選擇性氧化結果分析 74
4-3-2 改變電鍍時間之Ni-P裝載 81
4-3-2-1 基本性質分析 81
4-3-2-2 光電化學分析 86
4-3-2-3 選擇性氧化結果分析 88
4-3-3 交流阻抗頻譜 92
第五章、結論 97
第六章、未來建議 98
參考文獻 99
附錄 106

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指導教授

李岱洲(Tai-Chou Lee)

審核日期

2022-9-23

推文